Gas chromatography/time-of-flight mass spectrometry with time array detection, developed in the NIH-MSU laboratory, has led to a significant reduction in the analysis time required for volatile organic compounds (VOCs) by EPA method 524.2. Analyses previously requiring 30 40 minutes now require only 2 5 minutes for complete information recovery. With this fast analysis time, the primary obstacle to increased overall throughput is now the sampling process, typically requiring 10 15 minutes using purge and trap devices. The use of solid-phase micro-extraction is currently being examined as a more rapid sampling alternative, requiring only 5 minutes for adsorption and sample transfer. Our experiments thus far indicate that the combined SPME/GC-TOFMS instrumentation yields a significantly higher throughput than current conventional methodologies. Multiplexing of two SPME devices further increases the throughput to 5 minutes/sample. By both configurations, detectabilities below 10 ppb are achieved.